CN1800100A - Ceramet Ti3SiC2 powder preparation method - Google Patents

Abstract

The invention relates to a method of preparing metal ceramic Ti3SiC2 powder, belonging to chemo-composite material preparing technique field. The preparing steps are as follows: (1) select high-purity raw material of Ti, Si and C at the mole ratio of 3:1:2 as the basic chemical composition of preparing Ti3SiC2; add metal powder-Al as additive to control the degree of purity of Ti3SiC2 phase; the amount of Al is 10~50% mole of Si; (2) put said batches into non-corrodible steel ball grinder; add WC balls and said batches at the ratio of 20:1~30:1; charge argon gas, hematite, alloy mechanically; the revolution rate of ball grinder is 200~300rpm, the ball grinding time is 30~100 hours; (3) put the powder after alloying mechanically into pot to do annealing treatment at the atmosphere of argon gas with annealing temperature 850~1100 Deg C and annealing time 2~4 hours to get Ti3SiC2 powder. The degree of purity of production is said invention is high.

Description

Sintering metal Ti 3SiC 2The preparation method of powder

Technical field

The present invention relates to a kind of sintering metal Ti ₃SiC ₂The preparation method of powder belongs to the chemical synthetic material preparing technical field.

Background technology

Ti ₃SiC ₂It is the very promising ternary layered processable ceramics material of finding in recent years, it has the double properties of metal and pottery concurrently, it is as metal, it has favorable conductive, thermal conductivity under the room temperature, and lower microhardness and excellent heat-shock resistance are arranged, machinability, and at high temperature have plasticity; It is as pottery, and it has high elastic coefficient, high-melting-point, high chemical stability, high high-temperature machinery intensity and good antioxidant property.More meaningfully it has than lower frictional coefficient of traditional solid lubricant graphite and moly-sulfide and good self-lubricating property.Ti ₃SiC ₂Pottery has broad application prospects, and is the ideal candidates material of high-temperature engine, also can be used as the brush and the electrode materials of a new generation, also is fit to be manufactured on all kinds of anti-attrition members of working under high temperature, the chemical corrosion condition.Ti ₃SiC ₂Powder removes can be directly as original powder, and preparation has the Ti of excellent properties ₃SiC ₂Outside the block ceramic, also it can be come the high-temperature self-lubrication stupalith of synthesizing new as additive.

Although Ti ₃SiC ₂Have excellent performance, but prepare pure Ti ₃SiC ₂Block materials is difficulty very.Present Ti ₃SiC ₂The preparation method of block materials mainly contains chemical reaction, hot isostatic pressing, spreads certainly-hot isostatic pressing, discharge plasma sintering etc., has TiC powder, Ti in the product that most of preparation methods obtain usually ₅Si ₃, TiSi ₂Etc. phase, and need high temperature or long generated time usually, synthesis condition is comparatively harsh, and high preparation cost has limited the widespread use of this material in industry member.Consider from the angle that reduces cost, should adopt the pressureless sintering mode of being convenient to suitability for industrialized production to carry out the preparation of material as far as possible, and the synthetic active Ti of high-purity, high sintering ₃SiC ₂Powder is the key that realizes pressureless sintering.Consider Ti simultaneously ₃SiC ₂Can be used as additive and come the high-temperature self-lubrication stupalith of synthesizing new so Ti ₃SiC ₂The preparation of powder has received increasing concern in recent years.The preparation method also has solid-liquid reaction method, fluctuating synthesis method, combustion synthesis method etc. at present.Also have report to address mechanical alloying and add that the annealed method prepares, but processing condition are still undesirable, so still have a spot of TiC and Ti ₅Si ₃Impurity exists.

Summary of the invention

The object of the present invention is to provide and a kind ofly can control Ti ₃SiC ₂The preparation method of the sintering metal powder of thing phase purity.

A kind of sintering metal Ti of the present invention ₃SiC ₂The preparation method of powder is characterized in that having following preparation process and step:

A. took by weighing highly purified Ti, Si and C raw material in 3: 1: 2 in molar ratio, with this as the preparation Ti ₃SiC ₂Basic chemical ingredients; Other adds additive metal powder Al, with control Ti ₃SiC ₂The purity of thing phase; The add-on of additive metal powder Al is a benchmark with the molar weight of Si, promptly adds 10～50% of Si molar weight;

B. the raw material for preparing by said ratio is put into stainless steel jar mill; Add WC ball and above-mentioned admixtion by 20: 1～30: 1 weight ratio of ratio of grinding media to material in the ball grinder; Charge into argon gas subsequently, seal, and carry out mechanical alloying; The rotating speed of ball grinder is 200～300rpm, and the ball milling time is 30～100 hours;

C. the powder after the mechanical alloying is packed into and under argon shield, carry out anneal in the crucible; Annealing temperature is 850～1100 ℃, and annealing time is 2～4 hours; Cool to room temperature then with the furnace, products therefrom is sintering metal Ti ₃SiC ₂Powder.

Its purity height of the sintering metal powder that the inventive method makes can be used to prepare the block ceramic with excellent properties, and it has the two-fold advantage of metal and pottery concurrently, also can be with Ti ₃SiC ₂Come the high-temperature self-lubrication stupalith of synthesizing new as additive.The characteristics of the inventive method are to have added metal A l powder to control Ti ₃SiC ₂The purity of thing phase.Technology of the present invention is simple, easy handling, and low cost of manufacture.

Description of drawings

Fig. 1 is the X ray diffracting spectrum of the obtained powder of the inventive method.

Embodiment

After now embodiments of the invention further being described in.

Embodiment 1

The concrete preparation process and the step of present embodiment are as described below:

(1) 3: 1: 0.2 in molar ratio: 2 take by weighing purity greater than 99% Ti powder 6.9986g, purity greater than 99.99% Si powder 1.3681g, purity greater than 99.99% Al powder 0.2629g, and purity is greater than 99.99% C powder 1.1703g;

(2) will put into stainless steel jar mill by the admixtion that said ratio prepares; Add WC ball and above-mentioned admixtion by 20: 1 weight ratio of ratio of grinding media to material in the ball grinder; Charge into argon gas subsequently, seal, and carry out mechanical alloying; The rotating speed of ball grinder is 200rpm, and the ball milling time is 100 hours;

(3) powder after the mechanical alloying is packed under argon shield, carry out anneal in the crucible; Annealing temperature is 950 ℃, and annealing time is 2 hours; Cool to room temperature then with the furnace, products therefrom is sintering metal Ti ₃SiC ₂Powder.

Embodiment 2

The preparation process of present embodiment and step and the foregoing description 1 are basic identical.Its process and step are as follows:

(1) 3: 1: 0.5 in molar ratio: 2 take by weighing purity greater than 99% Ti powder 6.6009g, purity greater than 99.99% Si powder 1.2904g, purity greater than 99.99% Al powder 0.6199g, purity is greater than 99.99% C powder 1.1038g;

(2) will put into stainless steel jar mill by the admixtion that said ratio prepares; Add WC ball and above-mentioned admixtion by 30: 1 weight ratio of ratio of grinding media to material in the ball grinder; Charge into argon gas subsequently, seal, and carry out mechanical alloying; The rotating speed of ball grinder is 300rpm, and the ball milling time is 30 hours;

(3) powder after the mechanical alloying is packed under argon shield, carry out anneal in the crucible; Annealing temperature is 900 ℃, and annealing time is 2 hours; Cool to room temperature then with the furnace, products therefrom is sintering metal Ti ₃SiC ₂Powder.

Embodiment 3

The preparation process of present embodiment and step and the foregoing description 1 are basic identical.Its process and step are as follows:

(1) 3: 1: 0.5 in molar ratio: 2 take by weighing purity greater than 99% Ti powder 6.6009g, purity greater than 99.99% Si powder 1.2904g, purity greater than 99.99% Al powder 0.6199g, purity is greater than 99.99% C powder 1.1038g;

(2) will put into stainless steel jar mill by the admixtion that said ratio prepares; Add WC ball and above-mentioned admixtion by 30: 1 weight ratio of ratio of grinding media to material in the ball grinder; Charge into argon gas subsequently, seal, and carry out mechanical alloying; The rotating speed of ball grinder is 225rpm, and the ball milling time is 60 hours;

(3) powder after the mechanical alloying is packed under argon shield, carry out anneal in the crucible; Annealing temperature is 900 ℃, and annealing time is 2 hours; Cool to room temperature then with the furnace, products therefrom is sintering metal Ti ₃SiC ₂Powder.

The powder of gained in the foregoing description is carried out X-ray diffraction analysis detect, referring to the X ray diffracting spectrum of Fig. 1, from the characteristic peak of its existence as can be known, this powder is mainly Ti ₃SiC ₂Phase, its purity is very high.

Claims (1)

1. sintering metal Ti ₃SiC ₂The preparation method of powder is characterized in that having following preparation process and step:

A. took by weighing highly purified Ti, Si and C raw material in 3: 1: 2 in molar ratio, with this as the preparation Ti ₃SiC ₂Basic chemical ingredients; Other adds additive metal powder Al, with control Ti ₃SiC ₂The purity of thing phase; The add-on of additive metal powder Al is a benchmark with the molar weight of Si, promptly adds 10～50% of Si molar weight;

B. the raw material for preparing by said ratio is put into stainless steel jar mill; Add WC ball and above-mentioned admixtion by 20: 1～30: 1 weight ratio of ratio of grinding media to material in the ball grinder; Charge into argon gas subsequently, seal, and carry out mechanical alloying; The rotating speed of ball grinder is 200～300rpm, and the ball milling time is 30～100 hours;

C. the powder after the mechanical alloying is packed into and under argon shield, carry out anneal in the crucible; Annealing temperature is 850～1100 ℃, and annealing time is 2～4 hours; Cool to room temperature then with the furnace, products therefrom is sintering metal Ti ₃SiC ₂Powder.